C 1113 - 99 - Qzexmtm
C 1113 - 99 - Qzexmtm
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5.2 Estimates of heat flow, interface temperatures, and cold vs. time data, the rate of temperature change should preferably
face temperatures of single, and multi-component linings can be less than 0.05°C (0.09°F)/min. Four holes with alumina
be calculated using k-values obtained over a wide temperature protection tubes shall be provided in the kiln wall for the
range. platinum voltage and current leads. These holes should be
5.3 The k-values determined are “at temperature” measure- widely spaced to minimize electrical conductivity at elevated
ments rather than “mean temperature” measurements. Thus, a temperatures.
wide range of temperatures can be measured, and the results 6.1.2 Thermocouple, to measure sample temperature.
are not averaged over the large thermal gradient inherent in 6.1.3 Programmable Power Supply, capable of constant
water-cooled calorimeters. current control in the range from 0 to 10 A (0 to 50 V). During
5.4 The k-values measured are the combination of the a 10-min test period, stability should be 6 0.002 A. Size the
k-values for the width and thickness of the sample, as the heat power supply according to the anticipated wire harnesses
flow from the hot wire is in both of those directions. The diameter and type of materials to be tested. A high (5–10 A)
water-cooled calorimeter measures k-value in one direction, ampere supply is suggested for large diameter wire and/or
through the sample thickness. testing of high conductivity materials. However, lower ampere
5.5 The test method used should be specified when report- supplies will giver better current control for low currents used
ing k-values, as the results obtained may vary with the type of for low conductivity materials or with a smaller diameter wire
test method that is used. Data obtained by the hot wire method harness.
are typically 10 to 30 % higher than data obtained by the water 6.1.4 Shunt, with a resistance of 0.1 V rated at 15 A.
calorimeter method given in Test Method C 201. 6.1.5 Programmable Scanner, capable of directing several
different voltage inputs to the digital voltmeter. It is also used
6. Apparatus
to activate a relay to turn on and off the test circuit.
6.1 A block diagram of a suggested test apparatus is shown 6.1.6 Relay, with a current rating of 25 A at 24 V.
in Fig. 1. Details of the equipment are as follows:
6.1.7 Programmable Digital Voltmeter, with auto ranging,
6.1.1 Furnace, with a heating chamber capable of support-
auto calibration, and 6 1⁄2 digit resolution.
ing two 228-mm (9-in.) straight brick. The furnace temperature
6.1.8 Computer, capable of controlling the operation of the
may be controlled with a set point controller adjusted manually
power supply, scanner, and digital voltmeter. It must also be
between test temperatures, with a programmable controller, or
able to collect and analyze the test results. Commercially
with the computer. If a programmable controller is used, and
available data acquisition (with an IEEE device and sequential
the hot wire power is applied by computer, the furnace
file numbering capability) and analysis (spreadsheet with
temperature program must be synchronized with the computer
macro capability) software is acceptable; custom software is
program used to collect the test data. The furnace temperature
not necessary.
should be accurate to 6 5°C (9°F) and controlled to within a 6
1°C (1.8°F) precision such that the temperature variation with 6.1.9 Printer/Plotter, capable of documenting the raw data
time is minimized. Temperature stability measurements are not and various calculated values. The plotter function is used to
required by this test method because small temperature varia- plot the resistance versus ln (time) relationship. This is used to
tions with time are difficult to measure and dependent on visually determine if a linear relationship was obtained and the
thermocouple placement (in air, a protection tube, or in the location of the linear region.
sample). However, if sample temperature measurements are 6.2 Reusable Test Harness, consisting of a straight section at
averaged during a 30 minute period after furnace equilibration least 30-cm (11.8-in.) long with two perpendicular voltage
(prior to a hot wire test), the maximum-minimum difference leads about 15-cm (5.9-in.) apart near the center per Fig. 2. To
should preferably be less than 1°C (1.8°F). In addition, if a avoid thermocouple effect voltage errors, use pure platinum
linear regression analysis is done on the average temperature wire for the test harness, and for the entire length of voltage
leads. Platinum alloy wire may be used only for current leads
from outside the furnace to the test harness section itself. The
platinum voltage lead wires may be taken to an insulated
terminal box on the side of the furnace for connection to lower
temperature lead wires, or run all the way back to the digital
voltmeter terminals. The main part of the harness wire shall be
between 0.330 and 0.508-mm (0.013 and 0.020-in.) diameter.
The voltage leads may be the same size as the main harness
wire, although it is recommended that they be 0.330-mm
(0.013-in.) or smaller such that their area is less than half that
of the main wire. The current leads up to the main harness shall
be at least the same size as the main harness wire. The main
harness may be fabricated by butt welding voltage leads to a
solid main wire using a micro torch or arc percussion welder,
or by arc welding the wires into a bead. If beads are made by
arc welding, keep the bead size as small as possible, and
FIG. 1 Diagram of Apparatus carefully straighten out the bead to form a tee joint with the
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and voltage leads, it is permissible to chip out small cavities in
the brick at these locations using a hammer and center punch.
7.2.2 Refractory Castables—Refractory castables speci-
mens can be cut into brick shapes and prepared as in 7.2.1 or
a special castable mold with the 0.8-mm (0.032 in.) step can be
used to form the brick shapes. Two thin grooves must be cut for
the perpendicular voltage leads in one of the brick. The hot
wire harness can also be cast in place for a single usage.
7.2.3 Plastic Refractories and Ramming Mixes—
Immediately after forming, press the hot wire harness between
two 228-mm (9-in.) straight bricks. Pressure should be applied
during drying to keep the brick in very close contact.
7.2.4 Low-Strength Materials—Use a sharp knife to scribe
grooves into one of the brick into which the hot wire harness
will be pressed.
7.2.5 Compressible Refractory Fiber Blankets—Fabricate a
weighted cover to compress and hold the samples to the desired
thickness (and bulk density) during testing. A cover and side
spacers are required.
7.2.6 Powdered or Granular Materials—A refractory con-
tainer must be fabricated to contain powdered or granular
materials. The container may be of two parts each the size of
a 228-mm (9-in) straight brick. The lower part will have four
sides and a bottom. The upper part will have four sides only.
FIG. 2 Hot Wire Sample Setup Alternatively, a container of one part only may be used. The
one-part container will have the volume of two 228-mm (9-in)
voltage lead perpendicular to the main wire. brick. Record the weight and interior volume for use in
calculating the apparent bulk density of the test material.
7. Sampling and Specimen Preparation
7.1 The test specimens consist of two 228-mm (9-in.) 8. Calibration
straight brick or equivalent. Select these specimens for unifor- 8.1 Depending on the data analysis calculation method
mity of structure and bulk density. Bulk density should be used, it may be necessary to determine the resistance of each
determined in accordance with Test Method C 134. test harness at 0°C (32°F) (Ro). This can be done experimen-
7.2 The hot wire harness is positioned near the center of the tally by placing the harness in a plastic tray with a slurry of
two brick shaped specimens and in intimate contact with both crushed ice, and measuring the resistance using the same
either by using samples with a step diamond ground into the 4-wire method which is used for elevated temperature resis-
mating surface, by forming the sample around the harness, or tance measurements. An alternate method is to measure the
by deformation of soft samples. See Fig. 2 for a schematic of resistance of the harness at room temperature and calculate an
how the steps provide intimate lateral contact with both halves Ro value from RT/Ro5(a+b*T+c*T2) where the equation coef-
of the sample assembly. ficients are obtained from prior tests of the wire lot. Wire
7.2.1 Refractory Brick—The steps cut in the brick shall harness calibration at 0°C (32°F) is not required if the wire
have a maximum depth of 0.8-mm (0.032-in.), although lesser resistance vs. temperature measurement method is used.
depths can be used for wires smaller than the 0.508-mm
(0.020-in.) maximum wire size. To insure that samples do not 9. Setup Procedure
rock, the average depth of both steps shall be within 0.1-mm 9.1 Measure the hot wire length, L, to the nearest 0.025-cm
(0.004-in.) of each other. In addition, the mating surfaces shall (0.01-in.). This distance is measured between the voltage leads.
be flat to less than 0.1-mm (0.004-in.) as determined by the 9.2 Refractory Brick—Position the hot wire harness on the
following procedure. After the steps are ground, the bricks grooved brick. Place the other brick on top and slide them
shall be placed together with the steps touching each other to together to lock the wire into very close contact with both
check for any noticable rock or movement between the two bricks.
bricks; no visible movement is acceptable. Rock is most often 9.3 Low-Strength Materials—Press the hot wire harness
caused by the use of a grinding wheel which has a high spot in into the scribed grooves.
the center, causing a smaller step depth close to the step than 9.4 Compressible Refractory Fiber Blankets—Position the
across the rest of the mating surface. Dressing the wheel so that hot wire harness between the fiber samples. Several layers may
it is flat or that the side which forms the step edge is high will be necessary for thin samples.
normally provide acceptable results. After the step height and 9.5 Powdered or Granular Materials—If a two-part con-
mating surfaces are acceptable, voltage lead grooves shall be tainer is used, fill the lower part with sample material level to
cut across the high part of the step in one of the samples. To its top. Position the hot wire harness in the top center of the
accommodate the weld beads at the junctions of the main wire lower part. Place the upper container part in position and fill it
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with additional test material. If a one-part container is used, fill TABLE 1 Maximum Currents in Amps for 0.508 mm (0.020 in.)
it approximately half way with test material, install the hot wire WireA
harness through small holes drilled in the container, and °C (°F)
Density Typical Temperature 800 1200
complete the filling with test material. For either type sample kg/m3 (lb/ft3) Material 25 (77) 400 (753) (1472) (2192)
container, weigh the entire test setup and calculate the apparent
120 (7.49) Fiber Blanket 0.4 0.6 0.8 1
bulk density. 300 (18.7) Fiber Board 1 0.8 0.8 0.8
9.6 Place the assembled test specimens into the furnace 370 (23.1) Block Insulation 1 0.8 0.8 0.8
480 (30.0) 2000 Insulating Brick 1.2 0.8 0.6 0.6
chamber on two supports to ensure uniform heating and weld 640 (39.9) 2300 Insulating Brick 1.4 1 0.8 0.6
the voltage and current leads to the corresponding hot wire 800 (49.9) 2600 Insulating Brick 1.6 1.2 1 1
leads. A micro-torch is well suited for this. Compress soft fiber 960 (59.9) 2800 Insulating Brick 1.6 1.4 1.2 1
1000 (62.4) Al2O3 Powders 1.4 1 0.8 0.8
samples with a weighted cover to the desired thickness (and 1200 (74.9) Insulating Castables 2 1.4 1.2 1.2
bulk density). Position the thermocouple at the top center of the 1300 (81.1) Bubble Al2O3 Brick 3.6 2 1.6 1.4
test specimens. Pull excess voltage lead wire outside the 1500 (93.6) Foundry Sand (loose) 1.6 1.2 1.2 1.2
1500 (93.6) Foundry Sand (bonded) 2.8 1.6 1.4 1.2
furnace to minimize wire length inside which may pick up AC 1700 (106.1) Fused SiO2 3.2 2 1.8 1.6
noise from heating elements above 1000°C (1832°F). 2100 (131.0) Firebrick 3.6 2.4 1.8 1.6
2400 (149.8) Firebrick 4 2.4 2 1.8
10. Test Procedure 2500 (156.0) SiC Monolithics 6 4 3.2 reactsB
2600 (162.2) SiC Brick 8C 6 5 reactsB
10.1 Program the computer and any separate furnace con- 2700 (168.5) 60 % Al2O3 LC Castables 5 2.8 2.4 2
troller to obtain the desired test temperatures and soak times. 2900 (181.0) Bonded AZS or 80 % Al2O3 5 3.2 2.4 2
Heating rates below 180°C/h (324°F/h) are recommended for >3000 (187.2) >95 % Al2O3 8 4 3.2 2.8
>3000 (187.2) >95 % MgO 8C 5 4 3.6
all materials to avoid thermal shock damage to the furnace and >3200 (199.7) Cr2O3/MgO Brick 6 5 3.2 2.8
samples. Rates as slow as 55°C/hr (100°F/h) are preferred for >3200 (199.7) Fused AZS 5 3.2 2.8 2.4
castable test specimens (see Practice C 865). Once the desired >3200 (205.9) Zirconia Brick 3.2 2 1.8 1.6
A
test temperature is reached, soak for minimum of 4 h before For 0.406-mm (0.160-in.) wire, multiply above settings by 0.80 to obtain about
the same temperature rise; for 0.330-mm (0.130-in.) wire, multiply the above
beginning test measurements if the furnace is separately settings by 0.65.
controlled. Soak periods of 8 h may be required at lower B
Platinum wire will react with SiC at high temperature. Testing of SiC products
temperatures, especially for low conductivity materials. If the above 540°C (1000°F) may cause damage.
C
High conductivity materials give low R versus ln(t) slopes and may not give
furnace is controlled by a computer which is programmed to repeatable results if the k value exceeds 15 W/m·K (104 Btu·in./h·ft2°F).
check for thermal stability, the minimum soak period is not
required. At least four test temperatures (for example, room ture to rise gradually even though the furnace power is off, so
and three additional points) shall be used to generate data for wait periods longer than 1 h are desirable at this temperature.
curve fitting. For monolithic (unfired) materials, test the 10.5 Calculate the final test results after all elevated tem-
samples only during the initial heating cycle to obtain heating perature testing is completed so that RT data from the entire
curve data; other materials may be tested using either heating temperature range can be curve fit.
or cooling test points.
10.2 Measure the hot wire resistance at each test tempera- 11. Calculation
ture to the nearest 1.0 3 10–6 ohms using a low power input. 11.1 Regression Coeffıcients—Use a polynomial regression
This is best done by setting the test unit power supply for a analysis to curve fit the low power resistance or resistivity
0.1–0.2 A output and using the voltage drop across the standard (RT/Ro) versus temperature data to a polynomial equation of
resistor to accurately measure the current. The same method of the form a + b*T + c*T2 using data from a minimum of 4 test
measuring resistance should be used at all temperatures. temperatures (for example, room temperature and 3 elevated
10.3 Power the wire with a test current to obtain a maximum temperatures).
temperature rise (dT/dt) of 0.5°C/min (0.9°F/min). Power 11.1.1 The classical method is to use RT/Ro (resistance/
levels may be calculated by the computer or preselected for resistance at 0°C (32°F)) data, in which case Ro must be
each material and test temperature combination. Table 1 is measured or calculated. Since Ro will vary with use due to
provided as a guide for preselecting test currents. A maximum stretching or cold work of the wire, or both, it must be
current of 8 amperes at room temperature corresponds to a periodically remeasured using a 0°C (32°F) ice bath slurry, or
maximum power input of about 6 watts, or about 0.5 watts/cm recalculated from a room temperature measurement and pre-
(1.3 watts/in.) of wire. Close the test circuit, apply the current viously determined polynomial regression coefficients in ac-
for a period of 5 (high conductivity materials) to 10 (low cordance with the relation RT/Ro 5 a + b*T + C*T2. The
conductivity materials) min, and record the resistance versus advantage of using RT/Ro data is that the regression coefficients
time data with the computer at time intervals of 3 s or less. At are normalized and directly comparable to data from other
the end of the test period, open the test circuit and discontinue sources (for example, different runs of the same wire or data
data acquisition while the sample temperature re-equilibrates. from harnesses of different lengths or wire diameters).
10.4 Wait a minimum of 1 h for the sample temperature to 11.1.2 An alternate method is to curve fit only resistance
equilibrate, and then repeat the power test at least three times and temperature data. The advantage of this method is that all
at each test temperature. The same test current need not be used data are determined with the sample in place, eliminating the
for each test repetition, depending on the software utilized. At need for ice bath measurements of Ro, and eliminating han-
room temperature, there is a tendency for the furnace tempera- dling effects which cause subtle changes in resistance. Thus,
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this method is generally preferred for routine testing. The multiplying the W/m·K values by 6.93577.
disadvantage is that the resistance/temperature regression co- 11.4 Rate of Temperature Rise—For each test, calculate the
efficients require each experimental run to be made to elevated rate of temperature rise of the wire at a time of 1 min using Eq
temperatures, and that the coefficients will vary with harness 13 or Eq 16:
length and diameter. if:
11.2 Slope Calculation—Calculate the slope (B) of the RT RT 2
versus ln(t) plot from the linear region of each test using an Ro 5 a 1 bT 1 cT is the equation used, (9)
appropriate linear regression analysis method. The linear
region may be determined by computer analysis with software, then:
or by visual examination of the RT versus ln(t) plots. To avoid dRT
biasing the linear regression analysis toward the upper part of dT 5 Ro ~b 1 2cT!, and dRT 5 Ro ~b 1 2cT!dT (10)
where: the units are W/m·K in accordance with Section 3. If 14. Keywords
desired, calculate the k values in Btu·in./h·ft2·°F units by 14.1 hot wire; refractories; thermal conductivity
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